Classifications

• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
  • C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
  • C22B26/10—Obtaining alkali metals
  • C22B26/12—Obtaining lithium
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
  • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
  • C22B7/001—Dry processes
  • C22B7/002—Dry processes by treating with halogens, sulfur or compounds thereof; by carburising, by treating with hydrogen (hydriding)
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
  • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
  • C22B7/04—Working-up slag
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
  • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
  • C22B9/10—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals with refining or fluxing agents; Use of materials therefor, e.g. slagging or scorifying agents
• • C—CHEMISTRY; METALLURGY
  • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
  • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
  • C25B1/00—Electrolytic production of inorganic compounds or non-metals
  • C25B1/01—Products
  • C25B1/18—Alkaline earth metal compounds or magnesium compounds
  • C25B1/20—Hydroxides
• • C—CHEMISTRY; METALLURGY
  • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
  • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
  • C25B1/00—Electrolytic production of inorganic compounds or non-metals
  • C25B1/01—Products
  • C25B1/24—Halogens or compounds thereof
  • C25B1/26—Chlorine; Compounds thereof
• • C—CHEMISTRY; METALLURGY
  • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
  • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
  • C25B15/00—Operating or servicing cells
  • C25B15/08—Supplying or removing reactants or electrolytes; Regeneration of electrolytes
  • C25B15/081—Supplying products to non-electrochemical reactors that are combined with the electrochemical cell, e.g. Sabatier reactor
• • C—CHEMISTRY; METALLURGY
  • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
  • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
  • C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
  • C25C3/02—Electrolytic production, recovery or refining of metals by electrolysis of melts of alkali or alkaline earth metals
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
  • H01M10/00—Secondary cells; Manufacture thereof
  • H01M10/54—Reclaiming serviceable parts of waste accumulators
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
  • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
  • Y02P10/00—Technologies related to metal processing
  • Y02P10/20—Recycling
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
  • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
  • Y02W30/00—Technologies for solid waste management
  • Y02W30/50—Reuse, recycling or recovery technologies
  • Y02W30/84—Recycling of batteries or fuel cells

Definitions

• Lithium-ion batteries have indeed become the preferred source of electrical energy whenever high energy or high power is desired in applications where weigh or volume are at a premium. This growth will likely continue in the next years: the global capacity of lithium-ion batteries that will hit the market each year is expected to reach hundreds of gigawatt-hours by the late 2020's.
• cathode compounds include lithium cobalt oxide (LCO), lithium manganese oxide (LMO), lithium nickel manganese cobalt oxide (NMC), lithium iron phosphate (LFP), and lithium nickel cobalt aluminum oxide (NCA).
• LCO lithium cobalt oxide
• LMO lithium manganese oxide
• NMC lithium nickel manganese cobalt oxide
• LFP lithium iron phosphate
• NCA lithium nickel cobalt aluminum oxide
• Lithium is furthermore used in the electrolyte in the form of LiPFe. The current lithium consumption in lithium-ion batteries accounts for about half of total lithium production.
• Lithium is also used in other products such as lithium primary batteries, as well as in lithium-bearing glasses, ceramics, polymers, casting powders, alloys, greases, and pharmaceuticals.
• Lithium-ion batteries involve complex compounds often comprising particularly valuable metals such as nickel and cobalt.
• the research in the field of battery recycling has therefore been focusing on the recovery of these metals rather than on lithium.
• the literature describes several hydrometallurgical processes that use a variety of extraction and purification steps to recover nickel and cobalt from powders derived from lithium-ion battery waste.
• Lithium typically ends up diluted in the residual liquor of the last hydrometallurgical step. Often, this stream goes directly to the waste water treatment plant without any attempt to recover the lithium. In rare cases, lithium is nevertheless recovered by precipitation; this step generally offers only a low recovery yield, unless it is combined with an energy- intensive crystallization and evaporation step.
• the present invention solves this dilution problem by concentrating the lithium in the fumes of a smelting operation instead of in the slag. These fumes are formed in much smaller amounts compared to slag, thus offering a more interesting starting product for a hydrometallurgical process.
• the concentrated lithium fumes are moreover easily leachable, thereby facilitating the purification steps.
• This result is achieved by the addition of a suitable source of chlorides to the smelting furnace. It should be noted that the formation and fuming of lithium as LiCI, using CaCL as a source of chlorides, has been described in the context of the lithium recovery from spodumene. A process has indeed been described wherein finely comminuted spodumene is mixed with powdered CaCL, the mixture being then subjected to high temperature roasting in the solid phase.
• US 2,561,439 teaches a vacuum chlorination-roasting process of comminuted spodumene pelletized with CaCL. LiCI evolves, which is condensed and recovered.
• US 2,627,452 teaches a preliminary thermal conversion of alfa to beta spodumene, followed by addition of CaCL, and by a second heat treatment in a rotary kiln, wherein LiCI is formed and volatilized.
• This chlorination-roasting process has also been applied to a lithium-bearing slag obtained from reducing smelting processes for the recovery of metals from spent lithium batteries.
• a lithium-bearing slag obtained from reducing smelting processes for the recovery of metals from spent lithium batteries.
• This is shown in CN 107964593 A, wherein the solidified lithium- bearing slag is first crushed and then mixed with a metal chloride such as CaCL. Subsequently, the mixture is roasted, and the evolving LiCI captured.
• a multi- step process comprising the production of the slag via smelting, the solidification of the slag, its comminution, mixing it with fine CaCL, roasting of the mixture and capturing the LiCI is however both expensive and energy intensive.
• this patent application relates to a process for the concentration of lithium in metallurgical fumes, comprising the steps of:
• the process comprises at least one further step in which the halogen intermediate used for the fuming of Li halide from the molten slag is produced from the Li halide fumed from the molten slag, which is reacted under conditions sufficient to produce said halogen intermediate and a lithium product, and wherein halogen is selected from Cl, Br and I.
• the patent application relates to a process for the concentration of lithium in metallurgical fumes, comprising the steps of:
• halogen is selected from Cl, Br and I.
• the first and the second halogen intermediate do not need to have the same chemical form, as outlined further below. Key is, however, that the halide is advantageously re-used in the fuming step of the process.
• halogen intermediate is a gaseous halogen or gaseous halogen compound, in particular a compound selected from a halogen or a hydrogen halide, more specifically the halogen intermediate is selected from chlorine, bromine, iodine, hydrogen chloride, hydrogen bromide, hydrogen iodide and mixtures thereof.
• halogen intermediate is selected from chlorine, bromine, iodine, hydrogen chloride, hydrogen bromide, hydrogen iodide and mixtures thereof.
• a most straightforward choice is chlorine, hydrogen chloride or mixtures thereof.
• said halogen intermediate comprises a gaseous halogen or gaseous halogen compound, in particular a compound selected from a halogen or a hydrogen halide;
• the process comprises at least one further step in which the halogen intermediate used for the fuming of Li halide from the molten slag is produced from the Li halide fumed from the molten slag, which is reacted under conditions sufficient to produce said halogen intermediate and a lithium product, and wherein halogen is selected from Cl, Br and I.
• gaseous halogen or gaseous hydrogen halide is selected from chlorine, bromine, iodine, hydrogen chloride, hydrogen bromide, hydrogen iodide and mixtures thereof, with a straightforward choice being chlorine, hydrogen chloride or mixtures thereof.
• halogen intermediate more specifically of chlorides
• the halogen intermediate leads to the fuming of LiCI and can be performed during or after smelting of the metallurgical charge. During the smelting the slag and the alloy are formed. It is also possible to perform the fuming on the molten slag, either before or after it has been separated from the alloy, e.g. by tapping.
• the halogen intermediate may be fed to the furnace as part of the metallurgical charge, for example as part of the fluxing agents, or added separately to the liquid slag during or after smelting. If the halogen intermediate comprises a gaseous halogen or gaseous halogen compound it is advantageous if it is added separately to the liquid slag during or after smelting.
• the halogen intermediate may be an alkali halide, earth alkaline halide, a hydrogen halide, the halogen itself or combinations thereof. More specifically, the halogen intermediate may comprise calcium chloride and/or magnesium chloride, more specifically the halogen intermediate may consist of calcium chloride, magnesium chloride or combinations thereof.
• the halogen intermediate may comprise a gaseous halogen or hydrogen halide, more specifically the halogen intermediate may consist of halogen or a hydrogen halide.
• the halogen intermediate may comprise chlorine or hydrogen chloride, more specifically the halogen intermediate may consist of chlorine or hydrogen chloride.
• the halogen might be combined with hydrogen, in particular in the absence of hydrogen halide.
• the Li halide After fuming the Li halide is being collected, for example by combining the fumes with a solvent, such as passing the fumes through a solvent or spraying water into the fumes, thus transferring the Li halide into a solution in a solvent or solvent mixture, particularly in water as the solvent.
• a solvent such as passing the fumes through a solvent or spraying water into the fumes, thus transferring the Li halide into a solution in a solvent or solvent mixture, particularly in water as the solvent.
• Other possible means are common gas cleaning setups, such as using a scrubber for Li fumes.
• major part of the lithium is meant at least 50% by weight of the lithium entering the process.
• the metallurgical charge may comprise transition metals.
• the transition metals of most interest are iron, copper, nickel, and cobalt.
• the fumes may comprise, next to Li halide, one or more of the transition metals. Steps can be taken to remove these metals from the Li halide, which in general can be done by conventional means such as keeping the pH of the solvent in the e.g. scrubber neutral. Transition metals can also be removed from the Li halide by crystallization or solvent extraction of Li, precipitating or solvent extraction of the transition metals.
• the process is particularly suitable for concentrating lithium present in materials also containing nickel and/or cobalt.
• a pO 2 is then maintained that is sufficiently low to reduce a major part of at least one of nickel and cobalt to the metallic state, allowing these elements to report to the alloy phase.
• pO 2 stands for partial pressure of oxygen.
• major part is meant at least 50% by weight of the metals entering the process.
• oxidizing agents such as air or O2 and reducing agents.
• Typical reducing agents are natural gas or coal, but could also be metallic fractions like aluminum, elemental carbon, and plastics present in the metallurgical charge. Most preferred, however, is hydrogen. Carbon can also be employed.
• the redox potential can be determined by monitoring the yield of the metals such as nickel and cobalt to the alloy.
• Lithium which oxidizes easily, is assumed to quantitatively report to the slag. It will then react with the added chlorides, forming LiCI, which evaporates as fumes.
• the process is thus specially adapted for treating lithium-bearing materials comprising lithium batteries, their scrap, or their production waste.
• a hydrogen halide such as HCI can be used, either alone or in combination with a halogen, such as chlorine.
• a halogen such as chlorine.
• hydrogen is not needed, which avoids the handling difficulties with this highly volatile and flammable gas.
• Use of a H 2 /CI 2 burner to both create heat and HCI can be a suitable approach.
• the lithium-bearing material includes lithium cobalt oxide (LCO), lithium manganese oxide (LMO), lithium nickel manganese cobalt oxide (NMC), lithium iron phosphate (LFP), and lithium nickel cobalt aluminum oxide (NCA) or other battery materials containing lithium.
• LCO lithium cobalt oxide
• LMO lithium manganese oxide
• NMC lithium nickel manganese cobalt oxide
• LFP lithium iron phosphate
• NCA lithium nickel cobalt aluminum oxide
• Lithium is furthermore used in the electrolyte in the form of LiPFe.
• Lithium is also used in other products such as lithium primary batteries, as well as in lithium-bearing glasses, ceramics, polymers, casting powders, alloys, greases, slags and pharmaceuticals, which may also be present in the lithium-bearing materials.
• the lithium-bearing material may, for example, also contain nickel and/or cobalt.
• the lithium-bearing material comprises Li batteries, their scrap or their production waste.
• the halogen intermediate is added in an amount corresponding to a stoichiometric excess with respect to the Li in the fumes.
• An excess stoichiometric amount of halogen intermediate helps in these reactions to come as close to a quantitative yield as possible.
• the amount of halide that is added should thus preferably be at least stoichiometric with respect to lithium in the fumes. More preferably, a stoichiometric excess of more than 10 % is used.
• the amount of halogen intermediate is added should preferably be at least stoichiometric with respect to lithium in the slag. More preferably, a stoichiometric excess of more than 10 % is used. This will usually ensure a lithium fuming yield of more than 80%, or even of more than 90%.
• Suitable halogen intermediates are, for example, MgCL, more preferably CaCL. These chlorides have a high boiling point of respectively 1412 °C and 1935 °C at normal pressure, guaranteeing a good availability of these chlorides to react with the oxidized lithium in the slag at the operating temperature of the smelting furnace.
• Another option with good availability is a halogen, hydrogen halide or mixtures thereof, in particular chlorine, hydrogen chloride and/or bromine, hydrogen bromide and/or iodine and hydrogen iodide.
• the Li halide, in particular lithium chloride, that reports to the fumes can be separated and collected from the flue gas by using common unit operations, like scrubbers, baghouse filters, electro-static precipitators and cyclones.
• the process described here comprises at least one step in which the halogen intermediate used for the fuming of Li halide from the molten slag is produced from the Li halide fumed from the molten slag, which is reacted under conditions sufficient to produce said halogen intermediate and a lithium product.
• This step in which the halogen intermediate used for the fuming of Li halide from the molten slag is produced from the Li halide fumed from the molten slag has the technical effect to make the halogen of the lithium halide available to be used in the fuming in the form of the halogen intermediate, thus reducing salt load, waste materials and the need for adding expensive reagents.
• the step in which the halogen intermediate is produced comprises an aqueous electrolysis step or a molten salt electrolysis.
• the aqueous electrolysis step may comprise an electrolysis of an aqueous solution comprising the Li halide under conditions sufficient to obtain lithium hydroxide and the halogen intermediate that comprises hydrogen chloride, chlorine or mixtures thereof.
• the step in which the halogen intermediate is produced comprises a molten salt electrolysis.
• the molten salt electrolysis comprises an electrolysis of a salt melt comprising the Li halide under conditions sufficient to obtain lithium metal and the halogen intermediate, in particular chlorine.
• the step in which the halogen intermediate is produced comprises
• the aqueous electrolysis is an electrolysis of alkali halide to obtain alkali hydroxide and the halogen intermediate.
• the alkaline hydroxide can be converted to alkali carbonate by reaction with carbon dioxide.
• Said conversion reaction can be (a) a reaction of the Li halide with alkali hydroxide to alkali halide and lithium hydroxide, or (b) a reaction of the Li halide with an alkali carbonate to obtain lithium carbonate and alkali halide.
• Electrolysis often produces a halogen gas, more correctly a dihalogen gas such as chlorine gas (CI2), it can be combined with hydrogen to obtain hydrogen halide, such as, for example, hydrogen chloride (HCI) or other hydrogen halides like hydrogen bromide (HBr) or hydrogen iodide (HI).
• hydrogen halide such as, for example, hydrogen chloride (HCI) or other hydrogen halides like hydrogen bromide (HBr) or hydrogen iodide (HI).
• halogen as well as the hydrogen halide gas, individually or in combination, are suitable as halogen intermediate.
• chlorine or hydrogen chloride may be used as halogen intermediate as well as a mixture of chlorine with hydrogen chloride.
• the hydrogen halide can be reacted with alkaline or earth alkaline carbonates, hydrogen carbonates, oxides or hydroxides to form alkaline or earth alkaline halides that are suitable halogen intermediates, for example calcium chloride, magnesium chloride, sodium chloride or potassium chloride or other halides.
• Aluminum chloride can also be useful as halogen intermediate.
• Other alkaline or earth alkaline carbonates, oxides, hydrogen carbonates or hydroxides of barium, strontium, rubidium and cesium are also suitable, but usually aren't economically feasible.
• Ammonium hydroxide or ammonium carbonate can also be used instead of alkaline hydroxides or carbonates when appropriate.
• One embodiment for converting the Li halide into the lithium product and the halogen intermediate is a reaction sequence similar to the Solvay process.
• Another option is to react ammonia and carbon dioxide upfront to produce ammonium carbonate, and react lithium halide with the so produced ammonium carbonate
• ammonium halide can either be employed as halogen intermediate or reacted with calcium oxide to regenerate ammonia, calcium halide and water to produce calcium halide as halogen intermediate.
• Lithium hydrogen carbonate is heated to approx. 95°C, whereby water and carbon dioxide are released, producing lithium carbonate as the lithium product. This can be accomplished by calcination. Dependent on the reaction temperature of ammonium hydrogen carbonate with lithium halide, lithium carbonate can be obtained directly.
• lithium halide is reacted with ammonium carbonate, forming lithium carbonate directly.
• Ammonium carbonate can be prepared by reaction of carbon dioxide and ammonia in aqueous solution:
• ammonia is recovered, which - analogous to the Solvay process - is used again in the reaction with carbonic acid to form ammonium hydrogen carbonate and can thus be reused.
• ammonium chloride can either be employed as halogen intermediate or reacted with calcium oxide to form ammonia, calcium chloride and water to produce calcium chloride as halogen intermediate.
• a molten bath is then prepared in an alumina crucible of 2 L where 400 g of a starting slag is heated and melted in an induction furnace at a temperature of 1500 °C.
• This starting slag is the result of a previous operation and is used to provide a liquid bath to which the batteries can be added.
• the composition of the slag is given in Table 2.
• the batteries are added together with limestone and sand fluxes. The additions are made gradually over a period of 2 hours. During this time,
• O2 is blown at a rate of 160 L/hour above the bath to combust the metallic Al and carbon present in the batteries.
• the slag is allowed to react for an additional 30 minutes after the last CaCL addition, while still continuing the gas blowing with Ar. Samples of the slag are taken before the CaCL addition, after the final addition, and 30 minutes after the last addition. The results are shown in Table 3, together with the overall yield of the Li to the fumes.
• Table 4 Li content of the slag in function of time and stoichiometry (MgCL) NaCI was also tested as chlorinating agent, resulting in a yield of 26% when using a 100% stoichiometry. A super-stoichiometric addition of 250% NaCI result in satisfactory yields of 50% or more. This is shown in Table 5.
• the CaCI2, MgCI2 and NaCI halogen intermediates can be obtained by converting the CI2 and H2 gas produced during electrolysis to HCI and reacting the HCI with CaO, MgO and NaOH respectively.
• Table 6 Li content of the slag in function of time and stoichiometry (CI2) Samples of the fumes all show a lithium concentration of 15%, which corresponds to a LiCI content of more than 90%.
• a molten bath is then prepared in an alumina crucible of 2 L where 400 g of a starting slag is heated and melted in an induction furnace at a temperature of 1500 °C.
• This starting slag is the result of a previous operation and is used to provide a liquid bath to which the batteries can be added.
• the composition of the slag is given in Table 8.
• the batteries are added together with limestone and sand fluxes. The additions are made gradually over a period of 2 hours. During this time, O2 is blown at a rate of 220 L/hour above the bath to combust the metallic Al and carbon present in the batteries.
• Table 7 Composition of the batteries
• Table 8 Detailed material balance of the smelting operation before chloride addition
• the electrolysis setup comprised a membrane electrolysis cell with 100 cm2 active membrane area.
• a stainless steel mesh cathode and an IrO2-MMO anode were used.
• a Nation cation exchange membrane was placed between the anode and cathode compartment.
• Two bottles were connected to the anode and cathode compartments respectively and the electrolytes (anolyte and catholyte) were continuously circulated over the compartments with a flow rate of 200 mb/min using a peristaltic pump.
• the anolyte comprised 1 L of a 5 M LiCI solution.
• the catholyte comprised 300 mL of a 0.1 M LiOH solution.
• a small amount of LiOH was initially added to the catholyte to ensure a minimal electrolyte conductivity.
• the electrolysis cell was connected to a power supply and a current of 2.5 A was applied, corresponding to a current density of 250 A/m 2 .
• the electrolysis process was performed at room temperature (21 °C) for 28 h.
• Table 10 the volume and Li amount and concentration of the anolyte and catholyte before and after the experiment are indicated.
• Li was transferred from the anolyte to the catholyte compartment and converted to LiOH.
• a part of the water was transferred from the anolyte to the catholyte, which explains the decrease in anolyte volume and increase in catholyte volume.
• a catholyte LiOH concentration of 4.6 M was achieved, corresponding to a current efficiency for Li of 72%.
• the formation of both CI2 and H2 gas was demonstrated by gas analysis, which were re-used in the fuming reaction.

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